Gesellscitaft vur anilin fabrication



'ooloring-nntttor is oliizi' ilNiTEo @TATES FATENT @wicis.

.IOSEF STRASl-li Hill-CH, ()l MOSiOlY, .ltlSSlA, ASRI'GNOR TO 'll il AUTHEN- G ISELLSCHA'F' Fl R ANILIN FAl'lRIKA'llON, Oil BERLIN, GERMANY.

PRQCESS F WlAKlNG A BRGWN DYE.

SPECIFICATION forming part of Letters Fatent No. 399,581, dated March 12, 1889.

Application filed November 7, 1888. Serial No. 290,244. (No specimens.) Patented in Germany June 22, 1888, No. 1,939, and

July 14, 1888,170. 1,950; in England July 23, 1888, No. 10,053; in Russia July 30, 1888,110. 7,802; in France August 10, 1888, No. 179,276; in Austtimflungary August 10, 1888, No. 7,340, and in Italy September 80, 1888, XXII, 23,899,

XLVII, 206

To all, who/n, i l; III/fol] (fa/worn.-

Be it known tlmtl, .Tosnii H'rnAs'nunoun, oi Moscow, in the Russian. Empire, have invented newand useful Improvements in the Production of Brown Coloring-Mutter which Dyes Cotton without the Use oi? u idordztnt, tt'or which I have obtained Letters 'lzitent in ltul y, September 30, 1888, Vol. XXI l No. 23,890, and Vol. XLVII, No. 200, and For whioh l huw'o mode applications in tornmhy. .lnne 32, isss, No. A Lil-'33), and July Li. 1888, No. A i,.)t); l lnglund, July 33, i888,'.\o. d) i rnun-o, August 10,1888, No. iTnfilTti; ltnssiu. .luly iill, 1888, No. 7,802; Ausi riu-l lung'ury, August; it) lbSS,'No. it 7, 3-.iil;) and ,1. do liereliy dovlzirithat the following;- is it full, elm-tr, and exam. deseri 'itionoii' the invent ion, \.'lil(ll will onuhlo to make and use the sznne.

It is well known ilnti nu o'i'ztiig'o ooloringxmutter is obtained iiy vonihining' .totrumn ingunutter iroin totruzi -dinhenyk szilieylio aeichztnd resorein are dissolved in tour thousand liters of boiling water, with an addition of twenty-live kilos oi caustic soda, (of it)" diuzohenzolo-sulphonio uoid. snspenihjnl in about six hundred liters oif water, are slowly entered into the alkaline solution. 'lhus u coloring-nmttor is ohtuiood whii'h is soluhlo with dil'tieulty in wit tor. its precipitation is (,oinpleted by adding usolution oi ooninion salt. It dyes motion in deep hrown slnnlos withoutthe use oi? u znoi-dsnti. An iilentiml the intermodizite product iorniei'l hy one inoleoule oii' tetra-m-diphoiiyl and. one molecule mlieylie zu'id acts upon thooolorin g-nnitior l'ornnnl by one molecule porudizmobenzole-sulphonie :teid und one molecule rosorein.

To produce the new coloring-mutter by this method, thirty-six kilos oi the coloring-matter iiroin iittlittll;LZ0l)(HlZUl(5-HillilllUlllt; amid mid resorein are dissolved in one thousand liters oi water, and to this solutioi'i an equivalent quantity oi the intermediate product from ivtrnzo-diiihonyl urnd sztlioylio noid is added. 'lo prepare the intornimliuti-e produot-s. 18.5 kilos oi. honzidine ure dissolved by niezi-ns oi' i'orty-oio'ht kilos oi' inuridlii-v :ieid in eight hundred litorsoi' wzttor :ind dhtzotixod l y ill}; kilos oi.- nitrite oi soda. The solution oi? the (llitZOUtllliilUllllil isihen ontorodinioztsolution I oi title-on kilos of suliryliv iii-id. 'Foiirtoeirkiios oiruust ii'rd lil, (oilihinnn mid thirty kilos others skilled in the nrtto which it ztpnortziins oi' (wzu'honnte ol' sodu. in twelve hundred. liters of outer. After the mixture oi the intermediate ])l' )(lll(l ;ti1(l the zi itl\'(l:lllliil()li((l vol orino'nnzatior hzts stood for uliont twyonty-i'our hours, it. is hoztted,zind the so-iorined eolorin'gmutter precipitated by common suit, iili ered, pressed, and dried. .lt dyes oneotton deep yi-limv-in'own shzules without the use oi' 2t mordunt. iii in exam uple I the nurzuliitzobenzoio-sulphoni'o :tvid ,is re ihiced ll llit}i'it(ll2LZU lwuzolo-sulphonicuoiihtho resulting;coloringnnttit-er dyes more yellowisl'i-hrown shades.

.Ithdmp/ IL 'H in the iirst method of exttzlljllfl l the nurudiugaohenxolo-snlnhonii: acid is i'onl:n :-e ,l iiy tu'euty-iire kilos oif slplnt-nu-phthylninine-nionosul llninio zit-id, u. oloringnnitt'or is obtained whieh dyes cotton redlirown. An identicaleoloringr-nnittei'isifornied Bunnie.) A'ii'er cooling,twenty kilos of purziit the intermediate product from ietrzi-zo-diphenyl and sulioylii'v maid nets upon the coloringnnitter ironi ttl nlni (lltLZUlittj lliiiilttlll'lU- inonosulphouio zioid and rosoroin. The produi-tion ot the lntt'or (Ulllilflliilil requires 22.15 kilos of zit whit-nu ihtlrviztniine-inoimsulphoiiie maid, ii \P h nnd rod liters oi'\\ztter,iourt-een kilos ol' ninristiu maid, and (31) kilos of nitrite of sodium. The dim 1o compound thus lorined is entered into 5: solution oi 11.5 kilosoi' resoroin, tiventy -i-iix kilos oi en-ustie sods. (oi 4i)" Bunnie-Q and 7.5 kilos oi' mirhonute oil; sodium in three hundred ilk-(rs oi' wax-tor.

The different isomeric alpha-diazonaphthaline-1nonosulphonic acids show in regard to the described reaction an analogous behavior, an d 'th e correspon dine colorin g-matters do not differ very much in regal-die their shades in dyeing cotton with them.

If the diazonaphthaline lllOllOSlllPhOlllG acids are replaci-nl by the disnlphonic acids of the .UflplltiltiillO, no remarkable variation re carding th eir shades is observed. The isom crie sulphonic acids of the beta-diazoiiaphthalinc, if employed instead of the alpha-diazonaphthaline-sulphonic acids in the described reactions, yield. coloring-matters which dye cotton more of a yello\\-'-ln'own (oloririg-matters of similar shades are also obtained i[. the mono or disiilphonic acids of: diazoazobenzole or diazoazo-tolnol are employed instead of the dimenaphthaline-snlphonic acids. Finally, it may be stated that in each of the described combin ations the tetrazo-diphenyl may be replaced by tetrazo-ditolyl without any important change of the effect;

I clai1nl. The process herein described of prodncing coloring-matter for dyeing, the same consisting, first, in combining tetrazo-diphenyl with one molecule of salicylic acid,then combining with the product one molecule of resorcin, and finally combining with the product a diazobcimole-sulphonic acid and precipitating the dye or color, snbstantiz-il y as specified. W V 7 2. The process herein described oi? producin geoloring-matter for d yeing, tn:v sisting in treating resorcin with paradiazobel'izole-sulphonic acid, then dissolving the product in water, then adding to the solution the product obtained by the n1 of tetrazo-di )hcn.yl with salicylic aci Li-m1 allowing the mixture to stand a suitable period of time, and then heating it and adding com.- mon salt, by which the coloring-matter is precipitated, which is finally filtered, pressedand dried, substantia ly as specified.

JOSEF S'IRASBURGER.

\V it-messes:

(J. M. WERLE, E. C. DUFFY. 

